Synthesis Of Functionalized Magnetic Nanoparticles And Its Application In The Detection Of Trace Amounts Of Veterinary Drug Residues In Environmental Water

In the development process of human being, the widely usage of dyes, detergents, fertilizers, pesticides, veterinary drugs and other organic matter, indeed meet the diverse needs of human life and production, but caused a lot of problems at the same time, such as: environmental pollution, ecological unbalance, etc., which will eventually affect the normal life activities of human, animal and plant. Therefore, the real-time and effective monitoring of trace residues of organic pollutants in the environment in implement effective monitoring and treatment is of great significance in terms of human health. Current analytical technologies determining organic pollutants in environmental samples are challenged by extremely low level of the target analytes and very complex matrix with many interfering substances in samples. So developing quick and efficient sample preparation procedure of environmental samples has important significance. Wherein the magnetic solid phase extraction as a new solid phase extraction form developed rapidly in recent years, because of its high separation efficiency, high enrichment factor, less solvent consumption, good extraction effect, simple operation and environmental friendliness has been widely used in complex matrices pretreatment. This article is committed with synthesis of functional magnetic nanocomposites, which is used to extract trace organic pollutants in environmental water samples. The main research contents are as follows:1. A kind of magnetic nanoparticles Fe₃O₄/TiO₂ was prepared and characterized by scanning electron microscope（SEM）, X-ray diffraction（XRD）, Zetasizer Nano series nanoparticle size analyzer and etc. Using the material as a magnetic solid phase extraction sorbents and UV spectrophotometry as detector, a new method for the detection of trace ciprofloxacin in water was established. Effects of some factors on adsorption rate of ciprofloxacin were investigated, such as sample acidity, adsorption time and the dosage of adsorbent. The results showed that under the conditions of pH 5.0, adsorption time 6 min, dosage of the adsorbent 12 mg, the material has a good adsorption of ciprofloxacin, with 0.3 mol/L sodium hydroxide solution may well be desorbed. Under the optimum conditions, the limit of method detection was 20 μ g/L. The proposed method has been applied to the determination of ciprofloxacin in water with spiked recoveries of 97.13% 98.00 % and RSD of 2.02 % 3.78 %.2. A kind of magnetic nanoparticles Fe₃O₄/C was prepared with solvothermal/hydrothermal method and characterized by transmission electron microscope（TEM）, fourier transform infrared spectroscopy（FT-IR）, X-ray diffraction（XRD）, and etc. Using the material as a magnetic solid phase extraction sorbents and UV spectrophotometry as detector, a new method for the detection of trace crystal violet（CV） in water was established. Effects of some factors on adsorption rate of CV were investigated, such as adsorption time, sample acidity and the dosage of adsorbent. The results showed that under the conditions of adsorption time: 10 min, pH 8.0, temperature 25 ℃, the material has a good adsorption of CV, with ethanol-0.5 mol/L p-toluenesulfonic acid（9:1, V:V） solution may well be desorbed. Under the optimum conditions, the limit of method detection was 24 μ g/L. The proposed method has been applied to the determination of CV in Ganjiang river water with spiked recoveries of 105.82 % 108.42 % and RSD of 3.59 % 6.13 %.3. Fe₃O₄/C was prepared and the material was used as a magnetic solid phase extraction sorbents and HPLC-DAD as detector, a new method for the detection of trace crystal violet（CV） and malachite green（MG） in water was established. Effects of some factors on adsorption rate of CV and MG were investigated, such as sample acidity, adsorption time and the dosage of adsorbent. The results showed that under the conditions of pH 8.0, adsorption time 10 min, temperature 25 ℃, with acetonitrile-0.5 mol/L p-toluenesulfonic acid（9:1, V:V） solution may well be desorbed. Under the optimum conditions, the limit of method detection for CV was 1.16 μg/L, and MG was 1.98 μ g/L. The proposed method has been applied to the determination of CV and MG in Ganjiang river water with CV spiked recoveries of 96.05%¹03.16%, and RSD of 2.59%⁴.11%; and MG spiked recoveries of 97.30%¹02.39%, and RSD of 1.99%².27%.